Reaktionsgleichung
[CH3:1][C:2]1[C:7]([C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-])=O)=[CH:10][CH:9]=2)=[CH:6][C:5]([C:17]([NH:19][C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([C:26]([F:29])([F:28])[F:27])[CH:21]=2)=[O:18])=[CH:4][CH:3]=1.O1CCOCC1.O.[OH-].[NH4+].S(S([O-])=O)([O-])=O.[Na+].[Na+].NC1C=CC=CC=1>>[NH2:14][C:11]1[CH:12]=[CH:13][C:8]([C:7]2[C:2]([CH3:1])=[CH:3][CH:4]=[C:5]([C:17]([NH:19][C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([C:26]([F:27])([F:28])[F:29])[CH:21]=3)=[O:18])[CH:6]=2)=[CH:9][CH:10]=1Komponenten
7
Reaktionsbedingungen
- Temperatur
- 25 °C
Versuchsvorschrift
6-Methyl-4′-nitro-N-[3-(trifluoromethyl)phenyl]biphenyl-3-carboxamide was dissolved in 1,4-dioxane (10.00 mL, 0.1281 mol) and water (5.00 mL, 0.278 mol), and ammonium hydroxide (0.18 mL, 0.0045 mol) was added. To the reaction was added sodium dithionite (1.10 g, 0.00632 mol) and this mixture was stirred at 25° C. for 2 hours at which time HPLC analysis showed aniline formation. The reaction was extracted with ethyl acetate and the organic extracts were washed with water, saturated NaCl, dried (MgSO4) and concentrated in vacuo. MS (EI) m/z=371 (M+H).
Aufarbeitung
- extractionThe reaction was extracted with ethyl acetate
- washthe organic extracts were washed with water, saturated NaCl
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-1fcedce4e3c04c45a9efd8a4a77f8d19
- Quelldatensatz
- uspto-grants-2013_08
- Patentnummer
- US08513270B2
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